CN117790105B - Iron-silicon-chromium alloy soft magnetic material and preparation method and application thereof - Google Patents
Iron-silicon-chromium alloy soft magnetic material and preparation method and application thereof Download PDFInfo
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- 229910000599 Cr alloy Inorganic materials 0.000 title claims abstract description 45
- 239000000788 chromium alloy Substances 0.000 title claims abstract description 45
- 239000000696 magnetic material Substances 0.000 title claims abstract description 40
- XEVZIAVUCQDJFL-UHFFFAOYSA-N [Cr].[Fe].[Si] Chemical compound [Cr].[Fe].[Si] XEVZIAVUCQDJFL-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 82
- 239000000956 alloy Substances 0.000 claims abstract description 65
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 63
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 36
- 239000010703 silicon Substances 0.000 claims abstract description 36
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 239000003822 epoxy resin Substances 0.000 claims abstract description 21
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 21
- 229910000519 Ferrosilicon Inorganic materials 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 17
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- 238000005245 sintering Methods 0.000 claims abstract description 17
- 238000000748 compression moulding Methods 0.000 claims abstract description 16
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- 239000002904 solvent Substances 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 12
- 229910008458 Si—Cr Inorganic materials 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
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- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 4
- 238000004146 energy storage Methods 0.000 claims abstract description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 4
- -1 silicate ester Chemical class 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 14
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 13
- 229910052804 chromium Inorganic materials 0.000 claims description 13
- 239000011651 chromium Substances 0.000 claims description 13
- 229910052742 iron Inorganic materials 0.000 claims description 9
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 6
- GPXCORHXFPYJEH-UHFFFAOYSA-N 3-[[3-aminopropyl(dimethyl)silyl]oxy-dimethylsilyl]propan-1-amine Chemical group NCCC[Si](C)(C)O[Si](C)(C)CCCN GPXCORHXFPYJEH-UHFFFAOYSA-N 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- IWICDTXLJDCAMR-UHFFFAOYSA-N trihydroxy(propan-2-yloxy)silane Chemical compound CC(C)O[Si](O)(O)O IWICDTXLJDCAMR-UHFFFAOYSA-N 0.000 claims description 3
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 15
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 abstract description 8
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
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- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 3
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- 230000035699 permeability Effects 0.000 description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 2
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- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
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- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
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- LAQFLZHBVPULPL-UHFFFAOYSA-N methyl(phenyl)silicon Chemical compound C[Si]C1=CC=CC=C1 LAQFLZHBVPULPL-UHFFFAOYSA-N 0.000 description 1
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- Soft Magnetic Materials (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention belongs to the technical field of soft magnetic materials, and discloses an iron-silicon-chromium alloy soft magnetic material, a preparation method and application thereof. The preparation method comprises the following steps: adding ferrosilicon chromium alloy powder into a solvent to be uniformly dispersed, then adding sodium silicate or silicate ester and an amino end capping agent, stirring and uniformly mixing, and adding an acid catalyst under the stirring condition to carry out polymerization equilibrium reaction; filtering, washing and drying after the reaction is finished to obtain active MQ silicon resin coated alloy powder; and mixing the obtained active MQ silicon resin coated alloy powder with an epoxy resin binder solution, granulating, performing compression molding on the obtained granulated powder, and sintering to obtain the Fe-Si-Cr alloy soft magnetic material. The preparation method of the invention adopts the specific active MQ silicone resin to replace the conventional silica sol in-situ cladding alloy powder, has the advantages of stable cladding and good cladding effect, and can obviously improve the comprehensive application performance in the fields of photovoltaic, energy storage, new energy automobiles and the like.
Description
Technical Field
The invention belongs to the technical field of soft magnetic materials, and particularly relates to an iron-silicon-chromium alloy soft magnetic material, a preparation method and application thereof.
Background
The Fe-Si-Cr alloy powder is one kind of common alloy material with excellent magnetic performance and mechanical performance and may be used widely in electronic, communication, automobile, aviation, etc.
Although the ferrosilicon chromium magnetic powder has higher resistivity, the ferrosilicon chromium magnetic powder still has the problems of large eddy current and serious heat generation when being used at high frequency. With the increase of the requirements of electronic devices for high frequency and high conversion efficiency, it is important to increase the use frequency of materials and reduce the heat productivity of materials. In order to improve the service performance of the ferrosilicon chromium magnetic powder core under high frequency, insulating coating or internal crystallization is carried out on the surface of the alloy powder material, and insulating precipitated phases are added among particles so as to improve the resistivity of the ferrosilicon chromium magnetic powder core, reduce eddy currents among the particles and inside the particles of the alloy material, reduce loss, reduce heating and improve the energy conversion efficiency.
At present, silicon dioxide or titanium dioxide is mainly used for insulating coating on the surface of the alloy powder, and a corresponding coating method mainly adopts silica sol or titanium sol. The powder, the silica sol and the epoxy resin are mixed, granulated, formed and heat treated as described in CN 112530655A, so that the eddy current inside and among particles is small, the power consumption is reduced, and the requirements of the current device on high insulation, high frequency, high saturation magnetic flux density and low power consumption can be met. CN 104028750B discloses a high bonding strength insulating coating treatment method for a metal soft magnetic composite material, wherein the composite powder prepared by a sol-gel method has high bonding strength with magnetic powder particles, uniform and compact coating, controllable thickness of a coating layer, good oxidation resistance, high saturation magnetization and excellent magnetic property and mechanical property. However, although the bonding force between the insulating layer and the alloy powder can be improved by coating through a sol-gel method, the generated SiO 2 or TiO 2 coating layer has high brittleness and is easy to break in the compression molding process, so that the insulating coating effect is reduced; meanwhile, the SiO 2 or TiO 2 coating layer has poor compatibility with the bonding resin, so that the dispersibility or the bonding effect is poor, and the density and the application performance of the sintered final magnetic powder are affected.
The problem that the SiO 2 coating layer generated by the sol-gel method has larger brittleness can be solved to a certain extent through the organic silicon resin dipping coating or the mixed coating. Such as those described in our earlier applications CN 115588548A, CN 116825468A. However, the bonding force between the organic silicon resin and the alloy powder is low, so that the coating effect is not ideal, and multiple layers of coating are often needed by adopting multiple means; meanwhile, the bonding strength of the organic silicon resin to the alloy powder is low, so that the relative density of the sintered magnetic powder core is low. CN 115798854A discloses a method for combining a low-melting-point organic silicon resin (dimethyl silicone oil, amino silicone oil, ethyl silicate) as a vaporization coating agent with a coupling coating (silane coupling agent, aluminate coupling agent, titanate coupling agent). But the bonding force of the adopted low-melting-point organic silicon resin and the alloy powder is low (the bonding force of the ethyl silicate on the alloy powder in an unhydrolyzed state is low), high-temperature vaporization coating is needed, and the process is complex. In addition, the literature also discloses that the surface insulation treatment (Wang Dong and the like, the surface coating of the ferrosilicon chromium alloy magnetic powder and the influence of the ferrosilicon chromium alloy magnetic powder on the magnetic powder core performance are carried out by adopting the ethyl orthosilicate coating liquid, the silane coupling agent and the like, 2019-03-005, the strict and the like, the research on the influence of the temperature and humidity and the silane coupling agent on the ferrosilicon chromium alloy powder is carried out, 2023), but the problem that the brittleness of the generated SiO 2 coating layer is larger still exists in the ethyl orthosilicate coating, the hydrolysis self-polymerization tendency is strong by adopting the silane coupling agent, the resin agglomeration phenomenon is formed, and the coating effect is reduced.
Therefore, the preparation method of the iron-silicon-chromium alloy soft magnetic material with good insulating coating effect, simple process and low cost is a technical problem which needs to be solved by the technicians in the field.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the primary aim of the invention is to provide a preparation method of an iron-silicon-chromium alloy soft magnetic material. The preparation method of the invention adopts the specific active MQ silicone resin to replace the conventional silica sol in-situ cladding alloy powder, has the advantage of strong bonding force with the alloy powder, simultaneously avoids the defect of larger brittleness of the SiO 2 cladding layer, and has the advantages of good cladding effect and stable cladding. Meanwhile, by matching with specific bonding resin, the alloy powder coated with the active MQ silicon resin in situ can be subjected to chemical crosslinking reaction, so that the bonding effect is improved, the relative density of the sintered magnetic powder core is remarkably improved, and the comprehensive application performance of the sintered magnetic powder core is finally improved.
The invention also aims to provide the Fe-Si-Cr alloy soft magnetic material prepared by the method.
The invention also aims to provide application of the Fe-Si-Cr alloy soft magnetic material in preparation of electronic devices in the fields of photovoltaics, energy storage, new energy automobiles and the like.
The invention aims at realizing the following technical scheme:
a preparation method of an iron-silicon-chromium alloy soft magnetic material comprises the following preparation steps:
(1) Preparation of active MQ silicone resin coated alloy powder:
adding ferrosilicon chromium alloy powder into a solvent to be uniformly dispersed, then adding sodium silicate or silicate ester and an amino end capping agent, stirring and uniformly mixing, and adding an acid catalyst under the stirring condition to carry out polymerization equilibrium reaction; filtering, washing and drying after the reaction is finished to obtain active MQ silicon resin coated alloy powder;
(2) And (3) mixing the active MQ silicone resin coated alloy powder obtained in the step (1) with an epoxy resin binder solution, granulating, performing compression molding on the obtained granulated powder, and sintering to obtain the iron-silicon-chromium alloy soft magnetic material.
Preferably, the iron-silicon-chromium alloy powder comprises the following elements in percentage by mass: 4-7% of silicon, 3-6% of chromium and the balance of iron.
Preferably, the average particle size D50 of the ferrosilicon chromium alloy powder is 2-20 μm.
Preferably, the solvent is at least one of ethanol and isopropanol.
Preferably, the silicate is at least one of ethyl orthosilicate, methyl orthosilicate and isopropyl orthosilicate.
Preferably, the amino-capping agent is 1, 3-bis (aminopropyl) tetramethyl disiloxane.
Preferably, the acid catalyst is hydrochloric acid or sulfuric acid; the temperature of the polymerization equilibrium reaction is 30-60 ℃ and the time is 2-6 h.
Preferably, the mass ratio of the ferrosilicon chromium alloy powder, the solvent, the silicate and the amino end capping agent is 100:100-400:6-15:2-6.
Preferably, the epoxy resin binder solution refers to an acetone solution of an epoxy resin.
Preferably, the addition amount of the epoxy resin is 1-5% of the mass of the active MQ silicone resin coated alloy powder.
Preferably, the temperature of the compression molding is 50-100 ℃ and the pressure is 500-800 MPa; the sintering temperature is 600-900 ℃ and the sintering time is 10-120 min.
The Fe-Si-Cr alloy soft magnetic material is prepared by the method.
The iron-silicon-chromium alloy soft magnetic material is applied to the preparation of electronic devices in the fields of photovoltaics, energy storage, new energy automobiles and the like.
Compared with the prior art, the invention has the beneficial effects that:
(1) The invention adopts specific active MQ silicon resin to coat alloy powder, the MQ silicon resin is a compact ball with a double-layer structure, the inner layer of the MQ silicon resin is composed of a tetrafunctional Si-O unit network, the MQ silicon resin has stronger binding force with the alloy powder, the alloy powder can be uniformly and stably coated, and the outer layer of the MQ silicon resin is composed of a monofunctional Si-O unit. By adopting a specific amino end capping agent to carry out polymerization equilibrium reaction, active amino groups can be uniformly distributed on the surface of the coated alloy powder, and the active amino groups and an epoxy resin binder are subjected to curing reaction in the subsequent compression molding process, so that the bonding effect and uniformity between the alloy powder and the epoxy resin are remarkably improved, and the comprehensive application performance of the alloy powder is finally improved.
(2) According to the invention, the alloy powder is coated by adopting the specific active MQ silicon resin, so that the alloy powder has better toughness than the conventional SiO 2 coating, the crushing and separation of the coating in the compression molding process are effectively avoided, the insulating coating effect and the uniformity of the compression molding blank body structure are obviously improved, and the comprehensive application performance of the magnetic powder core obtained after the subsequent sintering is obviously improved.
Detailed Description
The present invention will be described in further detail with reference to examples, but embodiments of the present invention are not limited thereto.
Example 1
A preparation method of an iron-silicon-chromium alloy soft magnetic material comprises the following preparation steps:
(1) Preparation of active MQ silicone resin coated alloy powder:
100g of iron-silicon-chromium alloy powder (90 wt% of iron, 5.5wt% of silicon and 4.5wt% of chromium) with the average particle size D50 of 5.6 mu m is added into 200g of ethanol solvent to be uniformly dispersed, then 12g of tetraethyl orthosilicate and 4g of amino end-capping agent 1, 3-bis (aminopropyl) tetramethyl disiloxane are added to be uniformly stirred and mixed, the temperature is raised to 50 ℃, and 10g of 5mol/L hydrochloric acid catalyst solution is added under the stirring condition to carry out polymerization equilibrium reaction for 4h; and after the reaction is finished, filtering, washing and drying to obtain the active MQ silicon resin coated alloy powder.
(2) Mixing 100g of active MQ silicone resin coated alloy powder obtained in the step (1) with 13g of epoxy resin binder solution (acetone solution with the mass fraction of 20 percent), granulating, carrying out compression molding on the obtained granulated powder at the temperature of 80 ℃ and the pressure of 700MPa, and then heating to 750 ℃ for heat preservation and sintering for 60min to obtain the iron-silicon-chromium alloy soft magnetic material.
Example 2
A preparation method of an iron-silicon-chromium alloy soft magnetic material comprises the following preparation steps:
(1) Preparation of active MQ silicone resin coated alloy powder:
100g of iron-silicon-chromium alloy powder (89 wt% of iron, 7wt% of silicon and 4wt% of chromium) with the average particle size D50 of 4.8 mu m is added into 150g of ethanol solvent for uniform dispersion, then 6g of sodium silicate and 3g of amino end-capping agent 1, 3-bis (aminopropyl) tetramethyl disiloxane are added for uniform stirring and mixing, the temperature is raised to 45 ℃, and 10g of 5mol/L hydrochloric acid catalyst solution is added under stirring for polymerization equilibrium reaction for 4h; and after the reaction is finished, filtering, washing and drying to obtain the active MQ silicon resin coated alloy powder.
(2) Mixing 100g of active MQ silicone resin coated alloy powder obtained in the step (1) with 15g of epoxy resin binder solution (30% by mass of acetone solution), granulating, performing compression molding on the obtained granulated powder at 60 ℃ and 800MPa, heating to 900 ℃, and performing heat preservation and sintering for 30min to obtain the iron-silicon-chromium alloy soft magnetic material.
Example 3
A preparation method of an iron-silicon-chromium alloy soft magnetic material comprises the following preparation steps:
(1) Preparation of active MQ silicone resin coated alloy powder:
100g of iron-silicon-chromium alloy powder (91 wt% of iron, 5wt% of silicon and 4wt% of chromium) with the average particle size D50 of 4.5 mu m is added into 300g of isopropanol solvent for uniform dispersion, then 15g of isopropyl orthosilicate and 5g of amino end-capping agent 1, 3-bis (aminopropyl) tetramethyl disiloxane are added for uniform stirring and mixing, the temperature is raised to 55 ℃, and 10g of 5mol/L hydrochloric acid catalyst solution is added under the stirring condition for polymerization equilibrium reaction for 4h; and after the reaction is finished, filtering, washing and drying to obtain the active MQ silicon resin coated alloy powder.
(2) Mixing 100g of active MQ silicone resin coated alloy powder obtained in the step (1) with 5g of epoxy resin binder solution (acetone solution with the mass fraction of 40%), granulating, performing compression molding on the obtained granulated powder at the temperature of 100 ℃ and the pressure of 600MPa, and then heating to 600 ℃ to perform heat preservation and sintering for 120min to obtain the iron-silicon-chromium alloy soft magnetic material.
Comparative example 1
This comparative example was compared to example 1, using silicone resin believed to be more chemical ES-1023 (methylphenyl silicone epoxy) instead of reactive MQ silicone coating. The method comprises the following specific steps:
(1) 100g of iron-silicon-chromium alloy powder (90 wt% of iron, 5.5wt% of silicon and 4.5wt% of chromium) with the average particle size D50 of 5.6 mu m is added into 200g of ethanol solvent for uniform dispersion, then 16g of Xinyue chemical ES-1023 organic silicon resin is added for uniform stirring and mixing, and the organic silicon resin coated alloy powder is obtained after drying.
(2) Mixing 100g of the organic silicon resin coated alloy powder obtained in the step (1) with 13g of an epoxy resin binder solution (acetone solution with the mass fraction of 20 percent), granulating, carrying out compression molding on the obtained granulated powder at the temperature of 80 ℃ and the pressure of 700MPa, and then heating to 750 ℃ for heat preservation and sintering for 60min to obtain the Fe-Si-Cr alloy soft magnetic material.
Comparative example 2
This comparative example uses amino silicone oil instead of reactive MQ silicone resin coating as compared to example 1. The method comprises the following specific steps:
(1) 100g of ferrosilicon chromium alloy powder (90 wt% of iron, 5.5wt% of silicon and 4.5wt% of chromium) with the average particle size D50 of 5.6 mu m is added into 200g of ethanol solvent for uniform dispersion, then 16g of amino silicone oil is added, stirred and mixed uniformly, and dried to obtain the amino silicone oil coated alloy powder. The amino silicone oil coating alloy powder is found to have obvious oil precipitation adhesion, which proves that the coating effect is poor.
(2) Mixing 100g of the amino silicone oil coated alloy powder obtained in the step (1) with 13g of an epoxy resin binder solution (acetone solution with the mass fraction of 20 percent), granulating, carrying out compression molding on the obtained granulated powder at the temperature of 80 ℃ and the pressure of 700MPa, and then heating to 750 ℃ for heat preservation and sintering for 60min to obtain the Fe-Si-Cr alloy soft magnetic material.
Comparative example 3
This comparative example uses silica sol instead of reactive MQ silicone coating as compared to example 1. The method comprises the following specific steps:
(1) 100g of iron-silicon-chromium alloy powder (90 wt% of iron, 5.5wt% of silicon and 4.5wt% of chromium) with the average particle size D50 of 5.6 mu m is added into 200g of ethanol solvent to be uniformly dispersed, 16g of silica sol is then added, the mixture is stirred and uniformly mixed, the temperature is raised to 50 ℃, and 10g of 5mol/L hydrochloric acid catalyst solution is added under the stirring condition to carry out coating reaction for 4 hours; and after the reaction is finished, filtering, washing and drying to obtain the silicon dioxide coated alloy powder.
(2) Mixing 100g of the silicon dioxide coated alloy powder obtained in the step (1) with 13g of an epoxy resin binder solution (acetone solution with the mass fraction of 20 percent), granulating, carrying out compression molding on the obtained granulated powder at the temperature of 80 ℃ and the pressure of 700MPa, and then heating to 750 ℃ for heat preservation and sintering for 60min to obtain the Fe-Si-Cr alloy soft magnetic material.
Comparative example 4
This comparative example is compared to example 1, using silicate and aminosilane coupling agent instead of reactive MQ silicone coating. The method comprises the following specific steps:
(1) 100g of iron-silicon-chromium alloy powder (90 wt% of iron, 5.5wt% of silicon and 4.5wt% of chromium) with the average particle size D50 of 5.6 mu m is added into 200g of ethanol solvent to be uniformly dispersed, then 12g of tetraethyl orthosilicate and 4g of silane coupling agent KH550 (3-aminopropyl triethoxysilane) are added, uniformly stirred and mixed, the temperature is raised to 50 ℃, and 10g of 5mol/L hydrochloric acid catalyst solution is added under the stirring condition to carry out polymerization coating reaction for 4h; and after the reaction is finished, filtering, washing and drying to obtain silicon oxide and aminosilane coupling coated alloy powder.
(2) Mixing 100g of silicon oxide and aminosilane coupling coated alloy powder obtained in the step (1) with 13g of epoxy resin binder solution (acetone solution with the mass fraction of 20%), granulating, performing compression molding on the obtained granulated powder at the temperature of 80 ℃ and the pressure of 700MPa, and then heating to 750 ℃ for heat preservation and sintering for 60min to obtain the ferrosilicon chromium alloy soft magnetic material.
The iron-silicon-chromium alloy soft magnetic materials obtained in the above examples and comparative examples were tested for magnetic permeability (test using a precision electromagnetic analyzer 3260B at a test frequency of 10 MHz), insulation resistance (test using a volume surface resistivity tester), high-frequency loss (FE-2100 SA soft magnetic high-frequency BH tester) and density (archimedes' displacement density tester), and the test results are shown in table 1 below.
TABLE 1
As can be seen from the results in Table 1, the magnetic permeability of the iron-silicon-chromium alloy soft magnetic material is not obviously adversely affected by adopting the specific active MQ silicone resin coated alloy powder compared with the traditional organic silicone resin, linear silicone oil coated alloy powder and silica sol and/or silane coupling agent coated alloy powder. But can significantly improve the insulation resistance of the soft magnetic material and reduce the high frequency loss. The reason is that the inner layer of the specific double-layer compact structure of the MQ silicon resin has good binding force with alloy powder, and good coating effect on the alloy powder is realized through in-situ polymerization. Meanwhile, the MQ silicon resin overcomes the defect of large brittleness of the silica sol and silicate coating, and has better coating stability. In addition, the active amino groups uniformly distributed on the outer layer of the MQ silicon resin form good chemical bond combination with the epoxy resin binder, so that the mixing dispersion effect and the bonding effect of the active amino groups with the epoxy resin binder are enhanced, and the insulation coating effect and the tissue uniformity of the magnetic powder core obtained through final hot press molding and sintering are obviously enhanced. The improvement of the structural uniformity of the Fe-Si-Cr alloy soft magnetic material obtained by final sintering by the coating of the active MQ silicone resin is further demonstrated by the comparison of the density test results.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (9)
1. The preparation method of the iron-silicon-chromium alloy soft magnetic material is characterized by comprising the following preparation steps:
(1) Preparation of active MQ silicone resin coated alloy powder:
adding ferrosilicon chromium alloy powder into a solvent to be uniformly dispersed, then adding sodium silicate or silicate ester and an amino end capping agent, stirring and uniformly mixing, and adding an acid catalyst under the stirring condition to carry out polymerization equilibrium reaction; filtering, washing and drying after the reaction is finished to obtain active MQ silicon resin coated alloy powder;
(2) Mixing the active MQ silicon resin coated alloy powder obtained in the step (1) with an epoxy resin binder solution, granulating, performing compression molding on the obtained granulated powder, and sintering to obtain the Fe-Si-Cr alloy soft magnetic material;
The silicate is at least one of ethyl orthosilicate, methyl orthosilicate and isopropyl orthosilicate; the amino end-capping agent is 1, 3-bis (aminopropyl) tetramethyl disiloxane.
2. The method for preparing the iron-silicon-chromium alloy soft magnetic material according to claim 1, wherein the iron-silicon-chromium alloy powder comprises the following elements in percentage by mass: 4-7% of silicon, 3-6% of chromium and the balance of iron; the average particle size D50 of the ferrosilicon chromium alloy powder is 2-20 mu m.
3. The method for preparing the ferrosilicon-chromium alloy soft magnetic material according to claim 1, wherein the solvent is at least one of ethanol and isopropanol.
4. The method for preparing the ferrosilicon chromium alloy soft magnetic material according to claim 1, wherein the acid catalyst is hydrochloric acid or sulfuric acid; the temperature of the polymerization equilibrium reaction is 30-60 ℃ and the time is 2-6 h.
5. The method for preparing the ferrosilicon chromium alloy soft magnetic material according to claim 1, wherein the mass ratio of the ferrosilicon chromium alloy powder, the solvent, the silicate and the amino end capping agent is 100:100-400:6-15:2-6.
6. The method for preparing the ferrosilicon-chromium alloy soft magnetic material according to claim 1, wherein the epoxy resin binder solution is an acetone solution of epoxy resin; the addition amount of the epoxy resin is 1% -5% of the mass of the active MQ silicon resin coated alloy powder.
7. The method for preparing the iron-silicon-chromium alloy soft magnetic material according to claim 1, wherein the temperature of compression molding is 50-100 ℃ and the pressure is 500-800 MPa; the sintering temperature is 600-900 ℃, and the sintering time is 10-120 min.
8. An iron-silicon-chromium alloy soft magnetic material, characterized in that the soft magnetic material is prepared by the method of any one of claims 1-7.
9. The application of the Fe-Si-Cr alloy soft magnetic material in the preparation of electronic devices in the fields of photovoltaics, energy storage and new energy automobiles.
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| JP2006245173A (en) * | 2005-03-02 | 2006-09-14 | Sumitomo Metal Mining Co Ltd | Resin-bonding magnet composition, manufacturing method thereof, and resin-bonded magnet using the same |
| CN106380603A (en) * | 2016-09-09 | 2017-02-08 | 华南理工大学 | Bis-amino-containing MQ silicone resin, and preparation method and application thereof |
| CN115762945A (en) * | 2022-11-29 | 2023-03-07 | 横店集团东磁股份有限公司 | Iron-nickel magnetic powder core and preparation method thereof |
| CN115798854A (en) * | 2022-11-29 | 2023-03-14 | 江西悦安新材料股份有限公司 | Low-chromium antirust iron-silicon-chromium magnetic powder core and preparation method thereof |
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| JP2006245173A (en) * | 2005-03-02 | 2006-09-14 | Sumitomo Metal Mining Co Ltd | Resin-bonding magnet composition, manufacturing method thereof, and resin-bonded magnet using the same |
| CN106380603A (en) * | 2016-09-09 | 2017-02-08 | 华南理工大学 | Bis-amino-containing MQ silicone resin, and preparation method and application thereof |
| CN115762945A (en) * | 2022-11-29 | 2023-03-07 | 横店集团东磁股份有限公司 | Iron-nickel magnetic powder core and preparation method thereof |
| CN115798854A (en) * | 2022-11-29 | 2023-03-14 | 江西悦安新材料股份有限公司 | Low-chromium antirust iron-silicon-chromium magnetic powder core and preparation method thereof |
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